AmMay?i9oi.arm'}    Contributions  from  H,  M.  Gordin.  219 
loids,  I  propose  the  following  method  which  has  given  me  very  good 
results : 
Put  10  c.c.  of  the  fluid  extract  into  a  50  c.c.  measuring  flask  and  fill 
up  to  the  mark  with  a  2  per  cent,  solution  of  sulphuric  acid.  Add 
about  1  or  2  grammes  powdered  talcum,  shake  vigorously  a 
minute  or  two  and  filter  through  a  dry  filter.  By  means  of  a 
pipette  or  a  burette  transfer  25  c.c.  (=  5  c.c.  extract)  into  a  separating 
funnel  having  a  capacity  of  about  125  to  150  c.c.  Add  into  the 
separator  40  c.c.  of  a  mixture  of  three  volumes  of  ether  and  one 
volume  of  choloroform,  then  add  a  considerable  excess  of  a  10  per 
cent,  solution  of  potassium  hydrate,  and  shake  well  a  few  minutes. 
Set  aside  until  the  mixture  has  separated  into  two  layers.  There 
is  generally  no  emulsion  at  all.  Should  there  be  one,  the  addition 
of  a  little  more  potassium  hydrate  will  generally  destroy  it.  Draw 
off  the  lower  layer  into  a  second  smaller  separating  funnel,  add  to  it 
about  20  c.c.  of  the  same  ether-chloroform  mixture  and  shake  again 
a  few  minutes.  After  separation  into  two  layers,  draw  off  the 
lower  layer  into  a  beaker  and  carefully  pour  the  ethereal  liquid 
from  the  smaller  into  the  larger  separator.  Return  the  aqueous 
liquid  to  the  smaller  separator  and  shake  out  once  more  with  about 
20  c.c.  of  above  ether-chloroform  mixture.  When  the  liquids  have 
separated  into  two  layers,  draw  off  the  lower  layer,  which  can  now 
be  rejected,  and  carefully  pour  again  the  ethereal  liquid  from  the 
second  into  the  first,  larger  separator.  Now  add  into  the  separator 
1  gramme  of  calcined  magnesia,  and  shake  until  the  ethereal 
liquid,  upon  a  few  minutes'  standing,  separates  out  crystal  clear.  If 
it  does  not  become  perfectly  clear,  add  a  little  more  magnesia  and 
shake.  Now  filter  through  a  dry  filter  into  a  light  tared  flask, 
washing  the  separator  and  the  filter  repeatedly  with  ether,  and  dis- 
til off  the  ethereal  solvent  completely,  taking  care  to  prevent  loss 
by  spurting.1  Dry  the  flask  for  two  hours  at  I30°C,  and  after 
cooling  in  desiccator,  weigh.  The  weight  multiplied  by  twenty 
gives  the  per  cent,  of  total  alkaloids  in  the  extract. 
For  the  estimation  of  ether  soluble  alkaloids,  add  into  the  flask  a 
few  grammes  of  clean  coarse  quartz  and  then  10  c.c.  of  stronger 
ether,  then  give  the  flask  a  circular  motion  in  a  horizontal  plane 
till  all  adhering  matter  is  detached  from  the  sides  of  the  flask.  Now 
This  can  be  done  by  laying  the  flask  on  its  side. 
